#------------------------------------------------------------------------------ #$Date: 2025-08-18 23:52:38 +0100 (Mon, 18 Aug 2025) $ #$Revision: 301791 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/89/2008953.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2008953 loop_ _publ_author_name 'Lashgari, Kianosh' 'Norrestam, Rolf' '\%Akermark, Bj\"orn' _publ_section_title ; Bis(2,2'-bipyridine)(pyridine-2-carboxylate)ruthenium(II) hexafluorophosphate at 173K ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first IUC9900108 _journal_paper_doi 10.1107/S0108270199098881 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '[Ru (C6 H4 O2) (C10 H8 N2)2] P1 F6' _chemical_formula_moiety 'C26 H20 N5 O2 Ru1 1+, P1 F6 1-' _chemical_formula_sum 'C26 H20 F6 N5 O2 P Ru' _chemical_formula_weight 680.51 _chemical_name_common ; [bis(2,2'-bipyridine)(pyridine-2-carboxylato)ruthenium(II)] hexafluorophosphate ; _chemical_name_systematic ; [bis(2,2'-bipyridine)(pyridine-2-carboxylato)ruthenium(II)] hexafluorophosphate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90.00 _cell_angle_beta 107.67(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.373(7) _cell_length_b 11.078(7) _cell_length_c 16.788(8) _cell_measurement_reflns_used 22 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 24.530 _cell_measurement_theta_min 18.039 _cell_volume 2547(2) _computing_cell_refinement 'DIF4 (Stoe & Cie, 1985)' _computing_data_collection 'DIF4 (Stoe & Cie, 1985)' _computing_data_reduction 'REDU4 (Stoe & Cie, 1985)' _computing_publication_material 'PLATON98 (Spek, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.921 _diffrn_measured_fraction_theta_max 0.921 _diffrn_measurement_device_type ; STOE 4-circle diffractometer ; _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 8171 _diffrn_reflns_theta_full 30.03 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_min 1.64 _diffrn_standards_decay_% 10 _diffrn_standards_interval_time 360 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_T_max 0.919 _exptl_absorpt_correction_T_min 0.806 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(X-RED; Stoe & Cie, 1997)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'thin flake' _exptl_crystal_F_000 1360 _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.399 _refine_diff_density_min -1.194 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 370 _refine_ls_number_reflns 6867 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.001 _refine_ls_R_factor_all 0.062 _refine_ls_R_factor_gt 0.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0567P)^2^+3.8959P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.105 _reflns_number_gt 5097 _reflns_number_total 6867 _reflns_threshold_expression I>2\s(I) _cod_data_source_file qa0150.cif _cod_data_source_block QA0150 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Numerical' changed to 'numerical' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_original_formula_sum 'C26 H20 F6 N5 O2 P1 Ru1' _cod_database_code 2008953 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Ru1 0.267007(14) 0.008616(18) 0.115398(12) 0.01662(7) Uani d . 1 . . Ru P1 0.73637(7) 0.01010(10) 0.37607(6) 0.0395(2) Uani d . 1 . . P F1 0.7340(2) 0.1195(3) 0.4370(2) 0.0771(9) Uani d . 1 . . F F2 0.7405(3) -0.0990(4) 0.3174(2) 0.0954(12) Uani d . 1 . . F F3 0.6233(2) 0.0212(4) 0.3374(3) 0.1090(14) Uani d . 1 . . F F4 0.8498(2) 0.0071(4) 0.4139(4) 0.143(2) Uani d . 1 . . F F5 0.7200(5) -0.0817(3) 0.4407(2) 0.136(2) Uani d . 1 . . F F6 0.7506(4) 0.1045(5) 0.3111(3) 0.1353(18) Uani d . 1 . . F N1 0.32232(16) -0.0081(2) 0.24354(14) 0.0187(4) Uani d . 1 . . N C2 0.26556(19) 0.0437(3) 0.28571(16) 0.0203(5) Uani d . 1 . . C C3 0.2882(2) 0.0362(3) 0.37159(18) 0.0260(6) Uani d . 1 . . C H3 0.2462 0.0708 0.3994 0.034 Uiso calc R 1 . . H C4 0.3732(2) -0.0227(3) 0.41690(18) 0.0292(6) Uani d . 1 . . C H4 0.3905 -0.0287 0.4760 0.038 Uiso calc R 1 . . H C5 0.4321(2) -0.0723(3) 0.37385(19) 0.0277(6) Uani d . 1 . . C H5 0.4915 -0.1111 0.4035 0.036 Uiso calc R 1 . . H C6 0.40443(19) -0.0653(3) 0.28792(18) 0.0234(5) Uani d . 1 . . C H6 0.4445 -0.1021 0.2590 0.030 Uiso calc R 1 . . H C7 0.1783(2) 0.1139(3) 0.23238(17) 0.0236(5) Uani d . 1 . . C O8 0.17192(14) 0.12113(18) 0.15484(12) 0.0226(4) Uani d . 1 . . O O9 0.12222(16) 0.1603(2) 0.26584(14) 0.0344(5) Uani d . 1 . . O N21 0.19650(16) 0.0171(2) -0.01061(14) 0.0196(4) Uani d . 1 . . N C22 0.12022(19) -0.0605(3) -0.03955(16) 0.0205(5) Uani d . 1 . . C C23 0.0735(2) -0.0755(3) -0.12451(18) 0.0282(6) Uani d . 1 . . C H23 0.0207 -0.1305 -0.1433 0.037 Uiso calc R 1 . . H C24 0.1051(2) -0.0095(3) -0.18126(19) 0.0327(7) Uani d . 1 . . C H24 0.0757 -0.0207 -0.2396 0.043 Uiso calc R 1 . . H C25 0.1799(2) 0.0731(3) -0.15205(19) 0.0312(6) Uani d . 1 . . C H25 0.2009 0.1219 -0.1899 0.041 Uiso calc R 1 . . H C26 0.2238(2) 0.0834(3) -0.06682(18) 0.0248(6) Uani d . 1 . . C H26 0.2755 0.1397 -0.0471 0.032 Uiso calc R 1 . . H N21' 0.15930(15) -0.1203(2) 0.10309(14) 0.0189(4) Uani d . 1 . . N C22' 0.09308(19) -0.1269(2) 0.02599(16) 0.0201(5) Uani d . 1 . . C C23' 0.00545(19) -0.1887(3) 0.01160(17) 0.0233(5) Uani d . 1 . . C H23' -0.0401 -0.1909 -0.0429 0.030 Uiso calc R 1 . . H C24' -0.0150(2) -0.2471(3) 0.07756(19) 0.0251(6) Uani d . 1 . . C H24' -0.0748 -0.2891 0.0691 0.033 Uiso calc R 1 . . H C25' 0.0533(2) -0.2428(3) 0.15545(18) 0.0239(5) Uani d . 1 . . C H25' 0.0417 -0.2832 0.2014 0.031 Uiso calc R 1 . . H C26' 0.1391(2) -0.1790(2) 0.16612(17) 0.0213(5) Uani d . 1 . . C H26' 0.1857 -0.1765 0.2202 0.028 Uiso calc R 1 . . H N31 0.37594(17) -0.0892(2) 0.09280(14) 0.0210(4) Uani d . 1 . . N C32 0.4635(2) -0.0308(3) 0.11060(18) 0.0255(6) Uani d . 1 . . C C33 0.5479(2) -0.0925(3) 0.1127(2) 0.0386(8) Uani d . 1 . . C H33 0.6089 -0.0517 0.1279 0.050 Uiso calc R 1 . . H C34 0.5430(3) -0.2137(4) 0.0926(3) 0.0468(10) Uani d . 1 . . C H34 0.6006 -0.2574 0.0949 0.061 Uiso calc R 1 . . H C35 0.4533(3) -0.2709(3) 0.0692(2) 0.0414(8) Uani d . 1 . . C H35 0.4480 -0.3533 0.0526 0.054 Uiso calc R 1 . . H C36 0.3714(2) -0.2063(3) 0.0704(2) 0.0299(6) Uani d . 1 . . C H36 0.3099 -0.2458 0.0548 0.039 Uiso calc R 1 . . H N31' 0.36773(16) 0.1400(2) 0.11984(14) 0.0214(5) Uani d . 1 . . N C32' 0.4585(2) 0.0999(3) 0.12403(17) 0.0246(6) Uani d . 1 . . C C33' 0.5356(2) 0.1801(3) 0.1351(2) 0.0365(8) Uani d . 1 . . C H33' 0.5993 0.1510 0.1402 0.047 Uiso calc R 1 . . H C34' 0.5192(3) 0.3020(3) 0.1388(2) 0.0408(8) Uani d . 1 . . C H34' 0.5717 0.3575 0.1469 0.053 Uiso calc R 1 . . H C35' 0.4262(3) 0.3432(3) 0.1307(2) 0.0372(7) Uani d . 1 . . C H35' 0.4133 0.4272 0.1311 0.048 Uiso calc R 1 . . H C36' 0.3522(2) 0.2600(3) 0.12194(18) 0.0271(6) Uani d . 1 . . C H36' 0.2884 0.2881 0.1173 0.035 Uiso calc R 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru1 0.01214(10) 0.02258(11) 0.01474(10) -0.00218(8) 0.00347(6) 0.00043(8) P1 0.0287(4) 0.0583(6) 0.0336(5) 0.0063(4) 0.0126(3) -0.0043(4) F1 0.0694(19) 0.0647(18) 0.102(2) 0.0189(15) 0.0327(17) -0.0263(17) F2 0.091(2) 0.123(3) 0.092(2) -0.033(2) 0.058(2) -0.066(2) F3 0.0351(16) 0.122(3) 0.158(4) -0.0047(17) 0.013(2) -0.011(3) F4 0.0424(17) 0.126(3) 0.222(5) 0.0338(19) -0.016(2) -0.100(3) F5 0.297(7) 0.070(2) 0.071(2) 0.036(3) 0.100(3) 0.0197(18) F6 0.171(4) 0.152(4) 0.107(3) -0.046(4) 0.077(3) 0.022(3) N1 0.0147(9) 0.0227(11) 0.0175(10) -0.0039(8) 0.0028(7) 0.0000(8) C2 0.0174(12) 0.0249(12) 0.0182(12) -0.0031(9) 0.0047(9) -0.0024(9) C3 0.0286(14) 0.0289(14) 0.0215(14) -0.0027(11) 0.0090(11) -0.0020(10) C4 0.0338(16) 0.0341(16) 0.0170(13) -0.0037(12) 0.0038(11) 0.0031(11) C5 0.0241(14) 0.0300(15) 0.0245(14) -0.0002(11) 0.0007(11) 0.0072(11) C6 0.0176(12) 0.0268(14) 0.0240(14) -0.0007(10) 0.0034(10) 0.0013(10) C7 0.0192(13) 0.0291(14) 0.0215(13) -0.0003(10) 0.0049(10) -0.0032(10) O8 0.0181(9) 0.0278(10) 0.0212(10) 0.0035(7) 0.0051(7) 0.0003(7) O9 0.0253(11) 0.0489(14) 0.0292(12) 0.0078(10) 0.0086(9) -0.0081(10) N21 0.0154(10) 0.0266(11) 0.0171(10) -0.0003(8) 0.0052(7) 0.0012(8) C22 0.0163(12) 0.0271(13) 0.0170(12) -0.0008(10) 0.0034(9) -0.0016(10) C23 0.0236(14) 0.0369(16) 0.0214(14) -0.0015(11) 0.0025(10) -0.0043(11) C24 0.0304(15) 0.0485(19) 0.0174(13) -0.0009(14) 0.0045(10) -0.0004(12) C25 0.0268(15) 0.0459(18) 0.0231(15) 0.0015(13) 0.0110(11) 0.0066(12) C26 0.0177(12) 0.0360(15) 0.0223(14) -0.0008(10) 0.0085(10) 0.0035(11) N21' 0.0147(10) 0.0231(11) 0.0181(11) -0.0021(8) 0.0038(8) -0.0004(8) C22' 0.0161(12) 0.0243(12) 0.0182(12) -0.0002(9) 0.0026(9) -0.0005(9) C23' 0.0178(12) 0.0253(13) 0.0241(15) -0.0027(10) 0.0022(10) -0.0033(10) C24' 0.0181(13) 0.0245(13) 0.0330(15) -0.0033(10) 0.0079(11) -0.0026(11) C25' 0.0246(14) 0.0231(13) 0.0262(14) -0.0034(10) 0.0109(11) 0.0013(10) C26' 0.0207(13) 0.0240(13) 0.0185(12) -0.0024(10) 0.0052(9) 0.0008(9) N31 0.0191(11) 0.0278(12) 0.0179(11) 0.0009(8) 0.0081(8) 0.0027(8) C32 0.0196(13) 0.0380(16) 0.0208(13) 0.0005(11) 0.0089(10) 0.0016(11) C33 0.0222(15) 0.051(2) 0.046(2) 0.0036(14) 0.0162(14) 0.0048(16) C34 0.038(2) 0.050(2) 0.063(3) 0.0160(16) 0.0315(18) 0.0105(19) C35 0.053(2) 0.0317(17) 0.053(2) 0.0096(15) 0.0356(19) 0.0059(15) C36 0.0340(16) 0.0296(15) 0.0312(16) -0.0016(12) 0.0175(13) 0.0005(12) N31' 0.0169(10) 0.0288(12) 0.0177(11) -0.0068(8) 0.0040(8) 0.0009(8) C32' 0.0179(13) 0.0369(15) 0.0197(13) -0.0055(11) 0.0066(10) -0.0005(11) C33' 0.0243(15) 0.053(2) 0.0356(18) -0.0155(14) 0.0136(13) -0.0074(15) C34' 0.0397(19) 0.046(2) 0.0400(19) -0.0254(15) 0.0170(15) -0.0081(15) C35' 0.046(2) 0.0303(16) 0.0368(18) -0.0144(14) 0.0143(15) -0.0006(13) C36' 0.0281(15) 0.0277(14) 0.0237(14) -0.0032(11) 0.0054(11) 0.0012(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N1 Ru1 O8 78.82(9) yes N21 Ru1 N21' 78.95(10) yes N31 Ru1 N31' 78.99(10) yes N31 Ru1 N21 89.97(10) no N31' Ru1 N21 97.35(10) no N31 Ru1 N1 94.13(10) no N31' Ru1 N1 88.93(9) no N21 Ru1 N1 173.07(8) no N31 Ru1 N21' 102.04(10) no N31' Ru1 N21' 176.13(9) no N1 Ru1 N21' 94.71(9) no N31 Ru1 O8 170.91(9) no N31' Ru1 O8 95.02(10) no N21 Ru1 O8 97.63(9) no N21' Ru1 O8 84.39(9) no F5 P1 F3 89.0(3) no F5 P1 F4 93.6(3) no F3 P1 F4 176.6(3) no F5 P1 F6 178.5(3) no F3 P1 F6 89.8(3) no F4 P1 F6 87.5(3) no F5 P1 F2 88.7(2) no F3 P1 F2 91.9(2) no F4 P1 F2 90.3(2) no F6 P1 F2 92.2(3) no F5 P1 F1 90.7(2) no F3 P1 F1 89.1(2) no F4 P1 F1 88.72(19) no F6 P1 F1 88.4(2) no F2 P1 F1 178.8(2) no C6 N1 C2 118.3(2) no C6 N1 Ru1 127.9(2) no C2 N1 Ru1 113.78(18) no N1 C2 C3 122.0(3) no N1 C2 C7 115.4(2) no C3 C2 C7 122.6(3) no C2 C3 C4 119.3(3) no C5 C4 C3 118.4(3) no C6 C5 C4 119.8(3) no N1 C6 C5 122.1(3) no O9 C7 O8 125.9(3) no O9 C7 C2 119.0(3) no O8 C7 C2 115.1(2) no C7 O8 Ru1 115.56(18) no C26 N21 C22 118.0(2) no C26 N21 Ru1 126.21(19) no C22 N21 Ru1 115.55(18) no N21 C22 C23 121.9(3) no N21 C22 C22' 114.6(2) no C23 C22 C22' 123.5(3) no C24 C23 C22 119.1(3) no C23 C24 C25 119.2(3) no C26 C25 C24 118.8(3) no N21 C26 C25 122.9(3) no C26' N21' C22' 117.9(2) no C26' N21' Ru1 125.98(18) no C22' N21' Ru1 114.82(18) no N21' C22' C23' 122.0(3) no N21' C22' C22 114.7(2) no C23' C22' C22 123.3(2) no C22' C23' C24' 119.4(3) no C25' C24' C23' 118.6(3) no C24' C25' C26' 119.4(3) no N21' C26' C25' 122.7(3) no C36 N31 C32 118.7(3) no C36 N31 Ru1 126.3(2) no C32 N31 Ru1 114.67(19) no N31 C32 C33 121.0(3) no N31 C32 C32' 114.6(2) no C33 C32 C32' 124.4(3) no C34 C33 C32 119.6(3) no C35 C34 C33 119.3(3) no C34 C35 C36 118.9(3) no N31 C36 C35 122.3(3) no C36' N31' C32' 118.9(2) no C36' N31' Ru1 125.7(2) no C32' N31' Ru1 115.3(2) no N31' C32' C33' 120.8(3) no N31' C32' C32 113.9(2) no C33' C32' C32 125.2(3) no C34' C33' C32' 119.5(3) no C33' C34' C35' 119.6(3) no C34' C35' C36' 118.8(3) no N31' C36' C35' 122.2(3) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 N1 . 2.063(2) yes Ru1 O8 . 2.100(2) yes Ru1 N21 . 2.052(3) yes Ru1 N21' . 2.070(2) yes Ru1 N31 . 2.033(2) yes Ru1 N31' . 2.038(2) yes P1 F5 . 1.556(4) no P1 F3 . 1.561(3) no P1 F4 . 1.561(4) no P1 F6 . 1.568(4) no P1 F2 . 1.572(3) no P1 F1 . 1.593(3) no N1 C6 . 1.348(3) no N1 C2 . 1.359(3) no C2 C3 . 1.381(4) no C2 C7 . 1.516(4) no C3 C4 . 1.390(4) no C4 C5 . 1.382(5) no C5 C6 . 1.377(4) no C7 O9 . 1.226(3) no C7 O8 . 1.279(3) no N21 C26 . 1.344(4) no N21 C22 . 1.361(3) no C22 C23 . 1.390(4) no C22 C22' . 1.472(4) no C23 C24 . 1.382(4) no C24 C25 . 1.384(5) no C25 C26 . 1.382(4) no N21' C26' . 1.346(3) no N21' C22' . 1.356(3) no C22' C23' . 1.388(4) no C23' C24' . 1.389(4) no C24' C25' . 1.377(4) no C25' C26' . 1.386(4) no N31 C36 . 1.346(4) no N31 C32 . 1.365(4) no C32 C33 . 1.384(4) no C32 C32' . 1.471(4) no C33 C34 . 1.381(6) no C34 C35 . 1.382(6) no C35 C36 . 1.383(5) no N31' C36' . 1.350(4) no N31' C32' . 1.359(4) no C32' C33' . 1.389(4) no C33' C34' . 1.375(5) no C34' C35' . 1.380(5) no C35' C36' . 1.380(4) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139056803